CN111034813B - Preparation method of novel structured emulsion for improving oxidation stability of grease - Google Patents
Preparation method of novel structured emulsion for improving oxidation stability of grease Download PDFInfo
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- CN111034813B CN111034813B CN201911134883.4A CN201911134883A CN111034813B CN 111034813 B CN111034813 B CN 111034813B CN 201911134883 A CN201911134883 A CN 201911134883A CN 111034813 B CN111034813 B CN 111034813B
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
- A23D7/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
- A23D7/06—Preservation of finished products
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
- A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/522—Antioxidants; Radical scavengers
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- Edible Oils And Fats (AREA)
Abstract
The invention belongs to the technical field of emulsion oxidation resistance and preparation, and particularly relates to a preparation method of a novel structured emulsion for improving the oxidation stability of grease. The structured emulsion comprises the following components: grease, gel, surfactant and water. The preparation method comprises dissolving surfactant in water to obtain water phase A; placing the gel in oil to obtain oil phase B; heating the water phase A and the oil phase B, and placing the oil phase B in the water phase A to prepare primary emulsion C; homogenizing the primary emulsion C, and storing at crystallization temperature. The method for preparing the oil structured emulsion has the characteristics of simplicity, strong stability, good antioxidant effect, capability of loading large oil quantity and the like, and simultaneously, the oil and the gel generate structure-activity relationship through physical action, so that the micro and macro properties of the emulsion can be improved, and the oil structured emulsion has adjustability and inclusion property. The invention solves the problem that the oil in the emulsion system is easy to oxidize and rancidity, and provides a new idea and method for enhancing the oil oxidation resistance of the emulsion system.
Description
Technical Field
The invention belongs to the technical field of emulsion system preparation and grease oxidation resistance, and particularly relates to a preparation method of a novel structured emulsion for improving grease oxidation stability.
Background
The emulsion system not only can be conveniently absorbed by human bodies, but also is a good carrier and can carry functional substances, more and more products are presented in the emulsion system in daily life, such as margarine, plant protein beverage (soybean milk, peanut milk, coconut milk, almond juice and the like), probiotic emulsion and the like, and besides common food products, cosmetic products are presented in the emulsion system, such as shampoo, moisturizing milk, facial cleanser and the like. The products of the emulsion system have common characteristics, namely, the products comprise fat, and the properties of different fat are different due to different amino acid compositions and proportions, for example, liquid edible fat containing Omega-3 fatty acid is more and more favored by consumers because of the advantages of anti-inflammation, anti-thrombosis, anti-cardioversion, blood fat reduction, vasodilation, skin rejuvenation, health and the like, but the fat is easy to oxidize during storage to cause fat rancidity because of containing more unsaturated double bonds. "rancidity of fat" means that the fat is gradually hydrolyzed or oxidized by oxygen, water, light, heat, microorganisms and the like to deteriorate and rancidify, so that neutral fat is decomposed into glycerin and fatty acid, or unsaturated chains in the fatty acid are broken to form peroxide, and then the neutral fat is sequentially decomposed into low-grade fatty acid, aldehydes, ketones and other substances, so that peculiar smell and peculiar smell are generated, and some rancidification products also have carcinogenic effect.
At present, in order to prevent the oxidation of fats and oils in the emulsion system, it is common to add various antioxidants such as BHA, BHT, PG, TBHQ, TP, vitamin E, DLTP, TDPA, etc. in addition, or to carry functional substances having oxidation resistance such as curcumin, eucalyptus polyphenol, etc.
The above methods are all by means of chemical action to achieve the effect of enhancing the antioxidation of the emulsion, and also have the problems of high price or difficult preparation, poor effect and the like, so that a better method is needed to improve the antioxidation capability of the grease in the emulsion system. Meanwhile, with the wider research field of oil gel and the application of the oil gel in multiple fields of food by virtue of excellent functionality, for example, the Chinese patent document with the publication number of CN 110215416A discloses camellia oil gel emulsion and a preparation method thereof, and the physical stability of the camellia oil emulsion is improved by adding a gelling agent into an oil phase to prepare the emulsion, so that the bioavailability of the camellia oil is improved.
However, no research is provided on the method for preparing the structured emulsion with good antioxidant effect by utilizing which type of oil gel and how to regulate crystallization means.
Disclosure of Invention
Based on the problems, the invention provides a preparation method of a novel structured emulsion for improving the oxidation stability of grease. The structured emulsion solves the problems that the oil in the emulsion system is easy to oxidize and has poor flavor and the like. Structured emulsions have the following advantages: the preparation is simple, the gel has wide selection range, and the structure-activity relationship between the gel and the grease can be realized to improve the property of the emulsion. The antioxidant property is strong, and the bad flavor of the grease can be covered. Has strong stability and can be stored for a long time at the temperature of 30-40 ℃. Can generate stronger viscosity and has better application prospect in the fields of cosmetics, medicines and the like. Has adjustability and inclusiveness, namely, an antioxidant can be added into an emulsion system or an active substance with antioxidant function can be carried.
In order to realize the technical purpose, the scheme of the invention is as follows:
a method for preparing novel structured emulsion for improving the oxidation stability of grease,
the raw materials comprise the following components in percentage by mass:
30-50% of oil
The gel accounts for 2-20% of the weight of the oil phase
The surfactant accounts for 0.1-2.0% of the weight of the water phase
The balance of water;
the preparation method specifically comprises the following steps:
s1, dissolving a surfactant in water, and stirring until the surfactant is completely dissolved to obtain a water phase A;
s2, placing the gel into grease, heating and stirring to obtain an oil phase B;
s3, heating the water phase A and the oil phase B to the heating temperature of the gel;
s4, after heating, placing the oil phase B in the water phase A, and shearing and dispersing to prepare primary emulsion C;
s5, homogenizing the primary emulsion C to obtain emulsion D, and storing at a crystallization temperature to obtain a structured emulsion;
wherein the gel comprises one or more of beeswax, rice bran wax, candelilla wax, carnauba wax, stearic acid, monoglyceride, palmitic acid, ethyl cellulose, phytosterol, and oryzanol.
Preferably, in step S2, the oil includes one or more of fish oil, perilla seed oil, linseed oil, soybean oil, rice bran oil, sunflower oil, peanut oil, olive oil, grape seed oil, camellia oil, and sesame oil.
Preferably, in step S1, the surfactant comprises one or more of hydroxypropyl methylcellulose, tween-20, tween-60, tween-80, OP-7, OP-9, OP-10, sodium dodecyl sulfate, span-20. The best is the compound of an anionic surfactant, a cationic surfactant and a nonionic surfactant.
Preferably, in step S2, the oil or fat is an edible oil or fat.
Preferably, in step S5, the crystallization temperature of emulsion D is in the range of 4-40 ℃.
Preferably, in step S2, the gelling agent is a fully lipophilic gelling agent.
By utilizing the method for structuring the emulsion, antioxidant and thickening effects can be achieved without additionally adding an antioxidant and a thickening agent.
In summary, the method provided by the invention has the following advantages:
the structured emulsion prepared by the invention has strong stability and good antioxidant effect, can hide the bad flavor of the grease, solves the problem of easy oxidation and rancidity of the grease, improves the bioavailability of the grease, and provides a new idea and method for enhancing the antioxidation of the grease in an emulsion system.
Drawings
FIG. 1 is a graph of emulsion type identification (O/W or W/O);
FIG. 2: example 1 comparison of the stability of beeswax structured emulsions on storage at ambient temperature;
FIG. 3: example 1 beeswax structured emulsion was compared to control for oxidation resistance;
FIG. 4: example 2 macroscopic and microscopic comparison of stearic acid structured oils at different crystallization temperatures;
FIG. 5: example 2 different crystallization temperatures stearic acid structured emulsions were compared to a control for oxidation resistance;
FIG. 6: example 2 different crystallization temperatures stearic acid structured emulsions were compared to a control DSC test;
FIG. 7: example 3 different concentrations of stearic acid structured emulsion compared to a control for tack;
FIG. 8: example 4 monoglyceride structured emulsion versus control antioxidant comparison;
FIG. 9: comparing the morphology tests of stearic acid and beeswax structured emulsions with different concentrations and temperatures;
FIG. 10: 4 ℃, and comparing the oxidation resistance of the structured emulsion of monoglyceride with the concentration of 5 percent, stearic acid and beeswax;
among these, the examples mentioned: the control groups were: gel-free emulsion (4 ℃); the oxidation stability tests were all carried out by storage at a constant temperature of 37 ℃.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1 preparation of beeswax structurization:
accurately weighing 0.32g of hydroxypropyl cellulose and 0.16g of xanthan gum according to the mass ratio of 2:1, putting the hydroxypropyl cellulose and the xanthan gum into 60g of water, and stirring in a water bath (80 ℃) until the hydroxypropyl cellulose and the xanthan gum are completely dissolved to prepare a water phase A;
accurately weighing 2.0g of beeswax and 40g of linseed oil, heating and stirring at 80 ℃ for 5min to completely dissolve the beeswax to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, placing the emulsion D at the crystallization temperature (4 ℃) for storing for 24 hours to obtain the beeswax structured emulsion.
Example 1 formulation composition:
as can be seen from FIG. 1, the structured emulsion prepared is an oil-in-water emulsion.
As can be seen from fig. 2, when the emulsion is stored at room temperature for 60 days, the emulsion is also in a stable state without delamination, and no mildew occurs, so that the prepared structured emulsion is known to have strong stability and antibacterial property.
As can be seen from FIG. 3, the oxidation rate of the oil is significantly reduced compared to the control emulsion when the beeswax-structured emulsion with a concentration of 5% is stored for a longer period of time, so that the oxidation rate of the oil can be effectively reduced by the beeswax-structured emulsion.
In addition, 10% and 15% beeswax were tried, the higher the concentration the better.
Example 2 preparation of stearic acid structured emulsions at different crystallization temperatures:
accurately weighing 0.3g of hydroxypropyl cellulose and 0.3g of sodium dodecyl sulfate according to the mass ratio of 1:1, putting the hydroxypropyl cellulose and the sodium dodecyl sulfate into 60g of water, and stirring in a water bath (at 90 ℃) until the hydroxypropyl cellulose and the sodium dodecyl sulfate are completely dissolved to prepare a water phase A;
accurately weighing 6.0g of stearic acid and 40g of perilla seed oil, heating and stirring at 90 ℃ for 10min to completely dissolve the stearic acid to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, storing the emulsion D at the crystallization temperature (4 ℃, 20 ℃) for 24h to obtain the stearic acid structured emulsion.
Example 2 formulation composition:
as can be seen from fig. 4, when 15% stearic acid is used to form the oleogel, the oleogel can be formed at different storage temperatures on a macroscopic scale; microscopically, there is a difference in the size of crystals formed at different storage temperatures, with the largest crystal particles formed at 4 ℃ and the smallest crystal particles formed at 30 ℃, and thus the difference in storage temperatures also causes a difference in the properties of the oleogel.
As can be seen from fig. 5, the antioxidant capacity of the structured emulsion containing 15% stearic acid was significantly improved compared to the control when the structured emulsion was stored at different temperatures. The oxidation rate of the structured emulsion in a short period of time is higher than that of the control group because the stearic acid is added into the grease to be heated, and meanwhile, the difference of storage temperature has no obvious influence on the oxidation resistance of the emulsion.
As can be seen from fig. 6, stearic acid does form crystals in the emulsion system, forming a structured emulsion.
In addition, 5% and 10% stearic acid were tried, and the higher the concentration, the better the effect.
Example 3 preparation of different concentrations of stearic acid structured emulsions:
accurately weighing tween-800.44 g and 0.22g of sodium dodecyl sulfate according to the mass ratio of 2:1, putting the tween-800.44 g and the sodium dodecyl sulfate into 65g of water, and stirring in a water bath (75 ℃) until the water phase A is completely dissolved;
accurately weighing 1.75g, 3.5g and 5.25g of stearic acid and 35g of perilla seed oil, heating and stirring at 75 ℃ for 10min to completely dissolve the stearic acid to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, placing the emulsion D at the crystallization temperature (20 ℃) for storing for 24h to obtain the stearic acid structured emulsion.
Example 3 formulation composition:
as can be seen from FIG. 7, the structure-activity relationship between stearic acid and fats in the emulsion system enhances the viscosity of the emulsion system, and the emulsion viscosity increases with the increase of the stearic acid concentration. The structured emulsion can thus exert antioxidant and thickening effects without the additional addition of antioxidants and thickeners.
The invention takes the example that the system provided by the invention can play the effects of oxidation resistance and thickening without additionally adding an antioxidant and a thickening agent.
Example 4 preparation of monoglyceride structured emulsion:
accurately weighing 0.3g of hydroxypropyl cellulose and 0.3g of sodium dodecyl sulfate according to the mass ratio of 1:1, putting the hydroxypropyl cellulose and the sodium dodecyl sulfate into 60g of water, and stirring in a water bath (70 ℃) until the hydroxypropyl cellulose and the sodium dodecyl sulfate are completely dissolved to prepare a water phase A;
accurately weighing 6.0g of stearic acid and 40g of perilla seed oil, heating and stirring at 70 ℃ for 5min to completely dissolve monoglyceride to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, placing the emulsion D at the crystallization temperature (4 ℃) for storing for 24h to obtain the monoglyceride structured emulsion.
Example 4 formulation composition:
as can be seen from fig. 8, 9 and 10, the antioxidant capacity of the structured emulsion prepared by using monoglyceride as a gelling agent is significantly better than that of the control group. Meanwhile, the self property of the gel can influence the distribution of the gel in an emulsion system, and because stearic acid has a hydrophilic group and beeswax does not exist, stearic acid crystals in a stearic acid structured emulsion system are not only distributed in emulsion oil drops but also distributed in a dispersed phase, and beeswax crystals in beeswax the beeswax structured emulsion system are completely distributed in the emulsion oil drops, so that the difference of oxidation resistance is caused. The beeswax structured emulsion has the strongest oxidation resistance, the monoglyceride structured emulsion is the second time, and finally the stearic acid emulsion.
Example 5 preparation of phytosterol and beta-oryzanol structured emulsion:
accurately weighing 0.525g of hydroxypropyl cellulose, 0.35g of sodium dodecyl sulfate and 0. 200.175 g of tween-water according to the mass ratio of 3:2:1, putting into 70g of water, and stirring in a water bath (at 90 ℃) until the water phase A is completely dissolved;
accurately weighing 0.675g of phytosterol, 0.225g of beta-oryzanol and 30g of sunflower oil according to the mass ratio of 3:1, and heating and stirring at 140 ℃ for 8min to completely dissolve the phytosterol, the beta-oryzanol and the sunflower oil to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, storing the emulsion D at the crystallization temperature (4 ℃) for 24 hours to obtain the phytosterol and beta-oryzanol structured emulsion.
Example 5 formulation composition:
example 6 preparation of an ethylcellulose structured emulsion:
accurately weighing 0.84g of hydroxypropyl cellulose, putting the hydroxypropyl cellulose in 70g of water, and stirring in a water bath (at 90 ℃) until the hydroxypropyl cellulose is completely dissolved to prepare a water phase A;
accurately weighing 1.2g of ethyl cellulose and 30g of soybean oil, heating and stirring at 150 ℃ for 10min to completely dissolve the ethyl cellulose to obtain an oil phase B;
mixing the oil phase B with the water phase A, and preparing a primary emulsion C (10000rpm/1min) by using a high-speed shearing dispersion machine (AD 500S-P);
preparing emulsion D (100Mpa and three cycles) by placing the colostrum C in a high-pressure homogenizer;
and fifthly, placing the emulsion D at the crystallization temperature (4 ℃) for storing for 24h to obtain the ethyl cellulose structured emulsion.
Example 6 formulation composition:
the above description is only a preferred embodiment of the present invention, and all the embodiments have significantly better oxidation resistance than the control group, and are not intended to limit the present invention, and any minor modifications, equivalent substitutions and improvements made on the above embodiments according to the technical essence of the present invention shall be included in the protection scope of the technical solution of the present invention.
Claims (5)
1. A preparation method of novel structured emulsion for improving the oxidation stability of grease is characterized in that,
the raw materials comprise the following components in percentage by mass:
30-50% of oil
The gel accounts for 2-20% of the weight of the oil phase
The surfactant accounts for 0.1-2.0% of the weight of the water phase
The balance of water;
the preparation method specifically comprises the following steps:
s1, dissolving a surfactant in water, and stirring until the surfactant is completely dissolved to obtain a water phase A;
s2, placing the gel into grease, heating and stirring to obtain an oil phase B;
s3, heating the water phase A and the oil phase B to the heating temperature of the gel;
s4, after heating, placing the oil phase B in the water phase A, and shearing and dispersing to prepare primary emulsion C;
s5, homogenizing the primary emulsion C to obtain emulsion D, and storing at a crystallization temperature of 4 ℃ to obtain a structured emulsion;
wherein the gel comprises one or more of beeswax, rice bran wax, candelilla wax, carnauba wax, stearic acid, monoglyceride, palmitic acid, ethyl cellulose, phytosterol, and oryzanol.
2. The method of claim 1, wherein in step S2, the oil comprises one or more of fish oil, perilla seed oil, flax oil, soybean oil, rice bran oil, sunflower oil, peanut oil, olive oil, grape seed oil, camellia oil, and sesame oil.
3. The method of claim 1, wherein in step S1, the surfactant comprises one or more of hydroxypropyl methylcellulose, tween-20, tween-60, tween-80, OP-7, OP-9, OP-10, sodium dodecyl sulfate, and span-20.
4. The structured emulsion prepared by the method for preparing the novel structured emulsion for improving the oxidation stability of the grease according to claim 1.
5. Use of the structured emulsion of claim 4 to enhance the antioxidant properties of an emulsified system.
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| CN113678899B (en) * | 2021-08-03 | 2023-06-23 | 华南农业大学 | Oil gel-based emulsion with stable interface crystallization and preparation method and application thereof |
| CN114304283A (en) * | 2021-12-15 | 2022-04-12 | 华南理工大学 | Preparation method of food-grade double gel based on grease gel and hydrogel |
| CN114698843B (en) * | 2022-03-25 | 2023-05-12 | 华南农业大学 | Perilla seed oil microemulsion-hydrogel system and preparation method and application thereof |
| CN116098289A (en) * | 2022-12-30 | 2023-05-12 | 武汉轻工大学 | Preparation method of DHA-containing rice bran-based carrier |
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| CN103082032A (en) * | 2012-12-25 | 2013-05-08 | 江南大学 | Preparation method of beewax-based plastic fat |
| CN110215416A (en) * | 2019-06-06 | 2019-09-10 | 浙江大学 | A kind of camellia oil oleogel lotion and preparation method thereof |
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| CN103082032A (en) * | 2012-12-25 | 2013-05-08 | 江南大学 | Preparation method of beewax-based plastic fat |
| CN110215416A (en) * | 2019-06-06 | 2019-09-10 | 浙江大学 | A kind of camellia oil oleogel lotion and preparation method thereof |
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